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Hydrochloric Acid → HCID 178502873、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Methoxamine | HCID 6082 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Dimethyl N-cyanodithioiminocarbonate | HCID 66289 | — |
| 反応物 | HCID 178433288 | HCID 178433288 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178502873 | HCID 178502873 | — |
反応手順
A solution of methoxamine (7.0 g), prepared from the hydrochloride and potassium hydroxide in methanol (50 ml) and water (10 ml) was added to a solution of dimethylcyanodithioimidocarbonate (7.3 g) in methanol (40 ml) and stirred at room temperature for 60 hours. A solution of 4-methyl-5-[(2-aminoethyl)thiomethyl]imidazole (8.6 g) in methanol (30 ml) was added and the resulting solution was heated under reflux for 18 hours. Concentration followed by chromatographic purification on a column of silica gel with chloroform-methanol (10:1) as eluant and final recrystallisation from acetonitrile afforded the title compounds m.p. 155°-6°
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04347250 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-db29a31065ea4a9bba1787ca9a1d4937 |
| 出典メモ | uspto-grants-1982_08 |